EP1236042B1 - Standard sample composition and manufacture thereof - Google Patents

Standard sample composition and manufacture thereof Download PDF

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Publication number
EP1236042B1
EP1236042B1 EP00980195A EP00980195A EP1236042B1 EP 1236042 B1 EP1236042 B1 EP 1236042B1 EP 00980195 A EP00980195 A EP 00980195A EP 00980195 A EP00980195 A EP 00980195A EP 1236042 B1 EP1236042 B1 EP 1236042B1
Authority
EP
European Patent Office
Prior art keywords
standard sample
sodium
composition
weight
solvent
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP00980195A
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German (de)
English (en)
French (fr)
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EP1236042A1 (en
Inventor
Lars-Ove Sjaunja
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Individual
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Individual
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Priority to DK00980195T priority Critical patent/DK1236042T3/da
Publication of EP1236042A1 publication Critical patent/EP1236042A1/en
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Publication of EP1236042B1 publication Critical patent/EP1236042B1/en
Anticipated expiration legal-status Critical
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/02—Food
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T436/00—Chemistry: analytical and immunological testing
    • Y10T436/10—Composition for standardization, calibration, simulation, stabilization, preparation or preservation; processes of use in preparation for chemical testing
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T436/00—Chemistry: analytical and immunological testing
    • Y10T436/10—Composition for standardization, calibration, simulation, stabilization, preparation or preservation; processes of use in preparation for chemical testing
    • Y10T436/109163—Inorganic standards or controls
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T436/00—Chemistry: analytical and immunological testing
    • Y10T436/25—Chemistry: analytical and immunological testing including sample preparation

Definitions

  • the present invention relates to analysis of foodstuff and/or feedstuff in general, and in particular to a composition for a standard sample suitable for the calibration of analysis equipment.
  • the product claimed in EP 0 962 768 comprises a composition of a complexing agent, e.g. emulsifying salts and an alkali salt.
  • a complexing agent e.g. emulsifying salts and an alkali salt.
  • the product is dissolved in water and the foodstuff to be analyzed is mixed with the solution, and the mixture is milled in a suitable mill.
  • a homogeneous dispersion in liquid form results, having a milk-like appearance.
  • This dispersion is then readily analyzed by common methods, such as mid-infrared (MIR) spectroscopy, (see for example WO 81/02467) UV spectroscopy or chemical extraction methods, to mention some.
  • MIR mid-infrared
  • a reliable standard sample having a guaranteed long term stability, at least of the order of 1-12 months, preferably 24 months or more, which is easily dissolved, preferably instantly, in the medium used, commonly water, but also in other polar solvents e.g. di-methyl-sulphoxide (DMSO), and which enables an analysis of a complex material such as a foodstuff/feedstuff to be performed much faster than today.
  • medium used commonly water, but also in other polar solvents e.g. di-methyl-sulphoxide (DMSO)
  • DMSO di-methyl-sulphoxide
  • the object of the invention is therefore in a first aspect to provide a standard sample composition having the above mentioned properties.
  • This is achieved by the composition defined in claim 1, which essentially is a dry powder comprising a foodstuff (or feedstuff) of interest.
  • the water content of the foodstuff in native state is known.
  • a well defined amount of said foodstuff itself is comprised.
  • it has preferably known values of the content of specific substances of interest, e.g. fat, proteins, carbohydrates etc.
  • the water content of the sample composition is ⁇ 5% by weight of water on the basis of the total composition, preferably ⁇ 1% by weight, more preferably ⁇ 0,1% by weight, most preferably ⁇ 0,0 1 % by weight of the total composition.
  • the powder is a freeze-dried powder.
  • the standard sample composition is a frozen suspension of the components in the powder product of claim 1.
  • FIG. 1 shows the correlation between a reference chemical method and an IR method using the invention.
  • foodstuff shall be taken to include foodstuff (for human beings) and feedstuff or fodder (for animals).
  • precursor as used herein, we mean an intermediate product that is to be finally treated to arrive at the claimed formulation.
  • “native state” we mean the state of a foodstuff in which an analysis is to be performed thereon. Thus, it can be both raw or cooked meat, fresh or pasteurized milk, etc.
  • a precursor of the standard sample composition according to the invention is made by essentially the same method as disclosed in the above referenced EP 0 962 768. Namely, a combination of a complexing agent and an alkali salt is made by mixing the components in suitable proportions. The mixture is dissolved in water, and then a quantity of the foodstuff of interest, suitably cut in pieces, is added to the solution. Preferably a composition as disclosed in EP 0 962 768 is used.
  • It comprises as a complexing agent sodium citrate or one or more phosphates from the group consisting of sodium citrate, sodium di-hydrogenphosphate, di-sodium hydrogenphosphate, di-sodium di-hydrogen pyrophosphate, tri-sodium monohydrogen pyrophosphate, tetra-sodium pyrophosphate, penta-sodium triphosphate and sodium hexametaphosphate, phosphonic acids, NTA, EDTA, zeolites, e.g. Na-Al-silcate, and polycarboxylates, or combinations thereof.
  • phosphates from the group consisting of sodium citrate, sodium di-hydrogenphosphate, di-sodium hydrogenphosphate, di-sodium di-hydrogen pyrophosphate, tri-sodium monohydrogen pyrophosphate, tetra-sodium pyrophosphate, penta-sodium triphosphate and sodium hexametaphosphate, phosphonic acids
  • the composition comprises one or more substances selected from the group consisting of sodium or potassium soda (Na 2 CO 3 , K 2 CO 3 ), silicates e.g. sodium or potassium meta-silicate and optionally a hydroxide, e.g. sodium or potassium hydroxide.
  • sodium or potassium soda Na 2 CO 3 , K 2 CO 3
  • silicates e.g. sodium or potassium meta-silicate
  • optionally a hydroxide e.g. sodium or potassium hydroxide.
  • the foodstuff will have a known composition also in terms of the component thereof that is of interest for the analysis, in addition to that of water.
  • the fat content of the cheese to be used for the manufacture of the standard sample should be accurately known, by other analysis, e.g. by methods approved by AOAC, ISO or IDF.
  • any component of any foodstuff could be used as the basis for the standard sample, as long as it is possible to obtain an accurate analysis of the raw material, in respect of the component substance of interest.
  • the mixture is treated in a mill in order to comminute the pieces of the foodstuff, such that a dispersion or suspension is formed.
  • a special mill manufactured by L O Sjaunja AB, Uppsala, Sweden can be used. It is available under the trade name LOSMIXER.
  • mixers/mills may be used as long as they produce a sufficiently fine comminution of the foodstuff.
  • the criterion that the mill must meet is that it should be able to produce a fine dispersion with microparticles, where most of the dispersions are in a colloidal phase, or that the sedimentation rate is less than some mm per hour.
  • the fat In the case of fat, the fat must be in a homogenous emulsion insuring that fat does not separate out, giving a fat layer on the surface. Separated fat implies that it is difficult to take out a representative sample.
  • the grounding in the mill is performed during a time period of about 20-300 seconds, and the result is a dispersion (suspension) having mostly a milk-like appearance.
  • the particle size is preferably in the colloidal range or at least most of the organic particles should be in that range.
  • the average particle size should preferably be ⁇ 50 ⁇ m, more preferably ⁇ 10 ⁇ m, and most preferably ⁇ 1 ⁇ m.
  • the content in the foodstuff of the component or components of interest is not measured on the raw material but instead by analysis of the dispersion obtained by the milling operation.
  • the dispersion as obtained from the milling process can be frozen, and supplied to the end user in vial containing an accurately measured quantity. This is entirely within the inventive concept, but has the drawback that it needs to be kept under deep-frozen conditions.
  • the dispersion is subjected to a drying process in order to reduce the water content to ⁇ 5% by weight, preferably to ⁇ 1% by weight, more preferably to ⁇ 0,1 %, most preferably to ⁇ 0,01 % by weight.
  • the content of the component in the standard sample can be determined on the final end product, i.e. the (freeze) dried material.
  • the invention comprises an analysis procedure, wherein analysis equipment is calibrated or checked for reproducibility by employing a standard sample of the invention.
  • analysis equipment is calibrated or checked for reproducibility by employing a standard sample of the invention.
  • the content in the standard sample of the component of interest must be accurately known, but for reproducibility purposes it suffices to know that the standard sample composition itself is constant over time, such that a stock sample always will give the same result.
  • a commercial matured cheese of the age of approx. 6 months was used in this experiment.
  • the used cheese was gouda type cheese (Pr adjud).
  • the composition of the cheese was 31% by weight (m/m) fat, 25.4% by weight(m/m) protein, 1.0% by weight lactic acid, 1.1 % by weight sodium chloride (NaCl) and 39% by weight of water.
  • a total amount of 500 g of cheese was used. Due to the mixing capacity the mixing was repeated 50 times. Each time 10 g cheese was mixed with 90 g of LOSsolver solution (manufactured by L O Sjaunja AB, Uppsala, Sweden) in 60 sec.
  • LOSsolver solution manufactured by L O Sjaunja AB, Uppsala, Sweden
  • the homogenous dispersion was then freeze-dried (at a condensator temp. of -50°C, and a vacuum pressure of 0.07 hPa) in a freeze-dryer (Heto CD8, manufactured by Heto Lab Equipment A/S, Birkeröd, Denmark) to a dry-matter content >99% by weight (m/m).
  • the cheese powder was stored in chemical and thermal shock resistance bottles of Duran borosilicate glass. The samples were then stored in ambient temperature for 1.5 years. The cheese powder was easily dissolved in distilled water.
  • the powder was instantly dissolved into a homogenous solution (dispersion), only by mixing the powder with a spoon or similar.
  • a dispersion is obtained within say 10 seconds, preferably within 5 seconds. If some heating is performed, e.g. to 40°C, the dissolution will take place quicker.
  • the solution was made up by taking 6.9 g of cheese powder and 93.1 g of distilled water. These amounts means that the original concentrations are prepared.
  • the freeze dried cheese powder was than analyzed every month with infrared spectroscopy. The reproducibility between the determinations was excellent. The relative deviation was less than 1%, which means that the absolute deviation of the fat content was ⁇ 0.3%.
  • Standard samples of meat were prepared in the same way as for cheese.
  • a lean pig meat of the muscle m. longissimus dorsi was used in this preparation.
  • the composition of the meat was 1.6 % by weight fat, 23.1 % by weight protein, 1.2 % by weight ash and 74.2 % by weight water.
  • 10 g of meat was mixed and milled with 90 g of "LOSsolver meat" solution (manufactured by L O Sjaunja AB, Uppsala, Sweden) in a blender/mixer (LOSmixer, manufactured by L O Sjaunja AB, Uppsala, Sweden).
  • the solution was heated to 40°C, before added to the mixer.
  • the total mixing time was 2 minutes.
  • the meat dispersion had a high degree of foaming.
  • the foams were minimized by adding 100 ⁇ l of Antifoam A concentrate (manufactured by Sigma, Steinheim, Germany).
  • the homogenous meat dispersion was then freeze dried in a freeze dryer to a dry-matter content > 99 % by weight.
  • the meat powder was stored in the same manner as the cheese powder.
  • the meat powder was analyzed on the preparation day and after 2 months, with the same result. Although, the meat samples can be somewhat more difficult to bring to a dispersion than the cheese samples, also the meat sample can be said to dissolve "instantly" for the purposes of the invention.
  • the reproducibility between the two analysis occasions was within 1 % (relative).
  • the meat standard samples are intended to be stored for at least 1 year.
  • a blank solution was prepared by mixing 90 ml LOSsolver MeatTM , 10 ml of Milli-Q water and 20 droplets of Antifoam B. The pH was adjusted to 10.2 by adding appropriate amounts of concentrated HCl.
  • the instrument used an infrared spectrometer, Dairylab 2 from Multispec Limited, which is a single-beam instrument designed for direct determinations of milk products, was zeroed against water and each sample was analyzed twice. The blank solution was analyzed before and after the samples to discover possible instrumental drift during measurements. All solutions were temperatured to 40°C prior to analysis.

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  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Dairy Products (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)
  • Investigating Or Analysing Biological Materials (AREA)
EP00980195A 1999-11-23 2000-11-23 Standard sample composition and manufacture thereof Expired - Lifetime EP1236042B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DK00980195T DK1236042T3 (da) 1999-11-23 2000-11-23 Standardprövesammensætning og fremstilling deraf

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
SE9904229A SE518082C2 (sv) 1999-11-23 1999-11-23 Standardprovkomposition och livsmedelsanalys, metod för dess tillverkning och metod för analys av livsmedel
SE9904229 1999-11-23
PCT/SE2000/002305 WO2001038868A1 (en) 1999-11-23 2000-11-23 Standard sample composition and manufacture thereof

Publications (2)

Publication Number Publication Date
EP1236042A1 EP1236042A1 (en) 2002-09-04
EP1236042B1 true EP1236042B1 (en) 2005-05-25

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EP00980195A Expired - Lifetime EP1236042B1 (en) 1999-11-23 2000-11-23 Standard sample composition and manufacture thereof

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US (1) US7229830B1 (sv)
EP (1) EP1236042B1 (sv)
AT (1) ATE296443T1 (sv)
AU (1) AU1749001A (sv)
CA (1) CA2392001A1 (sv)
DE (1) DE60020391T2 (sv)
SE (1) SE518082C2 (sv)
WO (1) WO2001038868A1 (sv)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112394002B (zh) * 2020-12-01 2022-02-15 中国农业科学院作物科学研究所 谷物籽粒含水率检测的校正方法、装置和可读存储介质

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1981002467A1 (en) * 1980-02-19 1981-09-03 Foss Electric As N A method for quantitatively determining components in a sample

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3573062A (en) * 1967-05-24 1971-03-30 Mayer & Co Inc O Meat products
USH35H (en) * 1984-10-29 1986-03-04 The United States Of America As Represented By The Secretary Of The Army Freeze dried cooked meats
SE524702C2 (sv) * 1998-05-25 2004-09-21 L O Sjaunja Ab Produkt för dispergering av livsmedel för analytiska ändamål

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1981002467A1 (en) * 1980-02-19 1981-09-03 Foss Electric As N A method for quantitatively determining components in a sample

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
OOGHE W. ET AL: "Comparison of some additives used in the preparation of freeze-dried lemon juice candidate reference materials", FRESENIUS' JOURNAL OF ANALYTICAL CHEMISTRY, vol. 360, 29 September 1998 (1998-09-29), pages 445 - 448 *

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US7229830B1 (en) 2007-06-12
AU1749001A (en) 2001-06-04
CA2392001A1 (en) 2001-05-31
WO2001038868A1 (en) 2001-05-31
DE60020391D1 (de) 2005-06-30
ATE296443T1 (de) 2005-06-15
EP1236042A1 (en) 2002-09-04
SE518082C2 (sv) 2002-08-20
SE9904229D0 (sv) 1999-11-23
DE60020391T2 (de) 2006-02-02
SE9904229L (sv) 2001-05-24

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